Gravimetric Determination of Aluminium As Oxinate

EXPERIMENT 3:
GRAVIMETRIC DETERMINATION OF
ALUMINIUM AS OXINATE
DATE/DAY: 04/04/2023 (TUESDAY)
NAME OF INSTRUCTOR:
Dr Saiful ‘Arifin Bin Shafiee
PREPARED BY:
NAME MATRIC NO.

SITI RANIA BINTI NORAZLI SHAM 2213054
SITI NORHIDAYU BINTI MOHD ZAWAWI 2215088

INTRODUCTION
Tris(8-hydroxyquinolinato)aluminium, Al(C9H6NO)3 is the formula for the chemical

compound aluminium. Alq3, which is its abbreviation, was synthesized and purified to
98.5%. The coordinated interaction between Al3+ and O ion is more intense than that
between Al3+ and N ion, according to the analysis of Alq3's hydrogen nuclear magnetic
resonance (HNMR) spectra. In the Alq3 molecule, the AlO bond forms a covalent bond
with the two different geometric isomers, which are mer isomer and fac isomer. By
precipitating aluminium with 8-hydroxyquinoline in an ammoniacal solution that also
contains tartrate, cyanide, and hydrogen peroxide, aluminium may be identified. The
method makes the direct precipitation of aluminium in the presence of all the substances
normally found in the “mixed oxides'' commonly called R2O3 possible.
A quantitative technique called gravimetric analysis uses the substance to be

measured to be selectively precipitated out of an aqueous solution made by aluminium
solution, distilled water, 0.1M HCL, Tris(8-hydroxyquinolinato)aluminium, and
ammonium acetate. Filtration is used to separate the precipitate from the remaining
aqueous solution then drying and weighting are repeated many times in order to remove
water and maintain the weight value of the precipitate. The mass of the substance in the
original sample can be calculated assuming that the chemical composition of the
precipitate is known and that the precipitation reaction is complete. This experiment aims
to determine Aluminium as oxinate [Tris(8-hydroxyquinolinato)aluminium] using
gravimetric analysis and to assess the effect of water on the mass of the product.
MATERIAL AND APPARATUS
Table 1.1: Materials and Apparatuses Used In This Experiment.
No. Material No. Apparatus
1. 0.1M HCl solution 1. 500.00mL beaker
2. 2M CH3COOH solution 2. Buchner funnel
3. 2% oxine solution, C9H7NO 3. Buchner flask

(8-hydroxyquinoline)
4. 2M NH4CH3CO2 solution 4. Dropper
5. Distilled water, H2O 5. Measuring cylinder
6. Thermometer
PROCEDURE
1. 10cm3 of the aluminium solution was pipetted into a 500cm3 beaker.

2. 150cm3 of distilled water containing 1cm3 of 0.1M HCl was added and the
solution was warmed on a hot plate to 62°C for about 40 minutes. The
solution was stirred using a clean glass rod. The temperature of the solution
was monitored using a thermometer.
3. While the solution was stirred, 20cm3 of a 2% solution of oxine
(8-hydroxyquinoline) in 2M acetic acid was added into the same beaker. At
this point, the precipitate is not yet formed.
4. 25cm3 of 2M ammonium acetate solution was added into the beaker in a
dropwise manner. The supernatant was faintly green in appearance which
indicates complete precipitation as oxine was present in slight excess in
which enough oxine reagent had been added.
5. The solution in the beaker was left to cool with frequent stirring.
6. A petri dish and a filter paper were weighed on an analytical balance and the
mass was recorded in the table.
7. The filter paper was put in the Buchner funnel and moistened thoroughly
with distilled water.
8. The vacuum knob is turned to provide suction from the aspirator to the
Buchner flask through the rubber tubing.
9. The precipitate was filtered through a Buchner funnel.
10. The precipitate was washed thoroughly with distilled water on the Buchner
funnel until no more water was sucked down from the porous plate.
11. The precipitate along with the filter paper was moved onto a petri dish and
the petri dish was closed to preserve the precipitate mass.
12. The precipitate was dried at 117.0°C in a laboratory oven.
13. The precipitate was left to cool and weighed as Al(C9H6ON)3.
14. Drying and weighing cycles were repeated five times until a constant weight
of 38.7313g was obtained.
15. The concentration (g/dm3) of aluminium in the solution was calculated.
Aluminium oxinate contains 5.874% aluminium.
DATA AND OBSERVATION
After getting the aluminium oxinate solution, we must filter it to get the precipitate
that forms. To get rid of the water present in the precipitate, it must then be dried in the
oven laboratory at a temperature of 117.0°C. The precipitate was then cooled at room
temperature before being re-weighed with an analytical balance. This process is repeated
five times until the value becomes constant, signifying that the precipitate is water-free.
Remember that the weight of the petri dish and the filter paper is combined to create the
value obtained from the scales; to obtain the absolute weight of the precipitate, subtract
the value obtained from the weight of the petri dish and filter paper.
Mass of petri dish: 37.3328 g Mass of filter paper: 1.2649 g
Table 2.1: Measures of the weight of the product.
Mass of sample + petri dish + filter paper (g) Mass of sample (g)
Product 1 39.1885 0.5908
Product 2 38.8118 0.2141
Product 3 38.7385 0.1408
Product 4 38.7350 0.1373
Product 5 38.7317 0.1340
Product 6 38.7313 0.1336
Average mass of final product = ( 0.1340g + 0.1336g) / 2

= 0.1338 g
Al+3 + 3OxH → Al[Ox]3 + 3H+
n(Al[Ox]) = mass / Mr
= 0.1338 g / (459.43 g/mol)
= 2.9314 ×10-4 mol
1 mole of Al3+ produce 1 mole of Al[Ox], ratio 1:1
Therefore n(Al[Ox]) = n(Al3+)
Total volume of solution = 10 cm3 + 150 cm3 + 1 cm3 + 20 cm3 + 25 cm3
= 206 cm3 × (1 dm3 / 1000 cm3)
= 0.206 dm3
[Al[Ox]] = m/V = 0.1338 g / 0.206 dm3
= 0.650 g/dm3
[Al3+] = (5.874/100) × 0.650 g/dm3
= 0.0382g/dm3
Figure 1: The solution of aluminium oxine. Figure 2: Drying precipitate using laboratory
oven.
Figure 3: Drying process repeated. Figure 4: Final product of Aluminium Oxine.

DISCUSSION OF DATA
Reproducibility of a result refers to the consistency of measurement. Based on the

masses obtained in Table 2.1 after several cycles of drying and cooling, the
reproducibility of weight measurement made with the balance indicates that the balance
gives out accurate readings because the mean masses of the precipitate under the same
condition are equal. This has led to the determination of the true and corrected masses of
the precipitate after each drying and cooling cycle weighed on the analytical balance.
When using an analytical balance, there are some possible errors because of the
extremely sensitive nature of the analytical balance that can give out false results. For
starters, air currents can affect the intricate mechanisms of the analytical balance. Even
small changes in air pressure from ceiling fans, air conditioners, and open doors may
cause the analytical balance to show false measurements. Secondly, in most cases, faulty
measurements are a result of user error. For instance, a lab worker may calibrate the
analytical balance improperly which can affect the accuracy of the balance. This explains
why labs have strict procedures for maintaining atmospheric standards to ensure accurate
readings and reduce user error. Thirdly, a cluttered workspace may impact the accuracy of
the analytical balance. It is crucial that nothing is in contact with the analytical balance,
otherwise, it may cause inconsistencies in the readings. Unlike metal containers, plastic
and glass weighing bottles can bear electric currents. Static charges may result in
non-reproducible measurement readings.
It can be seen that in Table 2.1, the trend of the masses of precipitate going down
the table is decreasing. The first two products show the largest difference in the masses of
the precipitate, and the difference between the next products are decreasing as the cycles
of drying and cooling increase. The range of the mass of the precipitate is 0.4572g which
means that the precipitate has lost 0.4572g of water throughout the drying and cooling
cycles. After six cycles of drying and cooling, the constant mass of the precipitate
obtained is 0.1336g with an average of 0.1338g.
The calculated number of moles of obtained aluminum oxinate is 2.9314×10-4 mol.
From the calculated number of moles of aluminum and its volume, it was obtained that
the experimental concentration of aluminum oxinate is 0.650g/dm3.
CONCLUSION
At the end of the experiment, aluminum successfully has been determined as an

oxinate gravimetric method. The concentration of aluminum in the solution was found to
be 0.0642 g/dm3. Gravimetric analysis mistakes frequently have to do with the purity of
the isolated constituent. The compounds that precipitate tend to be very insoluble, and
incomplete precipitation produces very little error. In order to ensure the precipitation
was complete, the ammonium acetate must be added in a dropwise manner. The process
of drying and weighing should be repeated numerous times because even the smallest
drop of water can change the solid's mass and thus alter the concentration of aluminium
oxine that has already been calculated.
QUESTIONS
1. Draw the structure of the aluminum complex of oxine.
2. What is the purpose of the ammonium acetate in the experiment?
Ammonium acetate acts as a buffer and is a combination of a weak acid and weak base,
commonly used in the preparation of buffer solutions along with acetic acid. Ammonium
acetate is used to replace the cell buffers that contain the nonvolatile salts in the
preparation of samples for spectroscopy or mass spectroscopy.
3. How would you recover the oxine from the complex?
Many oxinates are soluble in organic solvents for example; chloroform.
4. Give some industrial uses of Al compounds.
- Al can be used as dry crystal,

- Help print out papers
- Can be used as a mordant in the dyeing process
- Can be used as a treating reagent in water.
5. Suggest another method to determine Al.
The thermometric titration.

REFERENCES
1. Carpenter, M.E. (2019) Errors in titration experiments, Sciencing. Available at:

https://sciencing.com/errors-titration-experiments-8557973.html
2. Chemistry Paper 3, 2019. (n.d.). Waeconline.org.ng.
https://waeconline.org.ng/e-learning/Chemistry/chem328jq1.html
3. Victoria Blackburn.(2023) What is a diprotic acid?, All the Science.

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EXPERIMENT 3:

DATE/DAY: 04/04/2023 (TUESDAY)

NAME MATRIC NO.

SITI NORHIDAYU BINTI MOHD ZAWAWI 2215088

Tris(8-hydroxyquinolinato)aluminium, Al(C9H6NO)3 is the formula for the chemical

A quantitative technique called gravimetric analysis uses the substance to be

Table 1.1: Materials and Apparatuses Used In This Experiment.

No. Material No. Apparatus

1. 0.1M HCl solution 1. 500.00mL beaker

2. 2M CH3COOH solution 2. Buchner funnel

3. 2% oxine solution, C9H7NO 3. Buchner flask

4. 2M NH4CH3CO2 solution 4. Dropper

5. Distilled water, H2O 5. Measuring cylinder

1. 10cm3 of the aluminium solution was pipetted into a 500cm3 beaker.

Mass of petri dish: 37.3328 g Mass of filter paper: 1.2649 g

Table 2.1: Measures of the weight of the product.

Average mass of final product = ( 0.1340g + 0.1336g) / 2

Figure 3: Drying process repeated. Figure 4: Final product of Aluminium Oxine.

Reproducibility of a result refers to the consistency of measurement. Based on the

At the end of the experiment, aluminum successfully has been determined as an

2. What is the purpose of the ammonium acetate in the experiment?

3. How would you recover the oxine from the complex?

Many oxinates are soluble in organic solvents for example; chloroform.

4. Give some industrial uses of Al compounds.

- Al can be used as dry crystal,

5. Suggest another method to determine Al.

The thermometric titration.

1. Carpenter, M.E. (2019) Errors in titration experiments, Sciencing. Available at:

3. Victoria Blackburn.(2023) What is a diprotic acid?, All the Science.

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